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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,567 records · Page 87
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Synthesis and characterization of novel Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} perovskite material and possible application as a cathode for low–intermediate temperature SOFCs

Highlights: • Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using sol–gel methods. • Material was thoroughly characterized using Raman, FTIR, XRD, HRTEM, SEM, and TGA. • Electrochemical performance showed the materials are a promising new cathode material for low temperature SOFC. - Abstract: A novel perovskite material, Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} was synthesized using a sol–gel technique. The materials were calcined at temperatures of 800 °C, 900 °C, and 1000 °C and then characterized using X-ray diffraction, Raman and infrared spectroscopy, high resolution transmission electron microscopy and scanning electron microscopy (SEM). The particle sizes and crystallite sizes increased with increasing calcination temperature and formed perovskite type materials with some separate magnetite and iridium oxide. The powders were used to assemble button cells using samarium doped ceria as the electrolyte and NiO/SDC as the anode materials. The electrochemical properties were investigated using a Fiaxell open flanges test set-up and a Nuvant™ Powerstat-05 potentiostat/galvanostat. The Ce{sub 0.8}Sm{sub 0.2}Fe{sub 0.9}Ir{sub 0.03}Co{sub 0.07}O{sub 3−δ} cathode material calcined at 1000 °C exhibited the most promising performance, with a maximum power density of 0.400 W/cm{sup 2}, a current density of 0.8 A/cm{sup 2}, and a corresponding area specific resistance of 0.247 Ωcm{sup 2} at 500 °C. The button cells were reasonably stable over15 h.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Multi-angle Precession Electron Diffraction (MAPED): A Versatile Approach to 4D-STEM Precession

Precession of a converged beam during acquisition of a 4D-STEM dataset improves strain, orientation, and phase mapping accuracy by averaging over continuous angles of illumination. Precession experiments usually rely on integrated systems, where automatic alignments lead to fast, high-quality results. The dependence of these experiments on specific hardware and software is evident even when switching to nonintegrated detectors on a precession tool, as experimental set-up becomes challenging and time-consuming. Here, we introduce multi-angle precession electron diffraction (MAPED): a method to perform electron diffraction by collecting sequential 4D-STEM scans at different incident beam tilts. The multiple diffraction datasets are averaged together postacquisition, resulting in a single dataset that minimizes the impact of the curvature and orientation of the Ewald sphere relative to the crystal under study. Our results demonstrate that even four additional tilts improved measurement of material properties, namely strain and orientation, as compared to single-tilt 4D-STEM experiments. We show the versatility and flexibility of our MAPED approach with data collected on a number of microscopes with different hardware configurations and a variety of detectors.

4D-STEM↗
DOE OSTI2019

Characteristics and Tribological Behaviors of TiAlN/Cr-Ni Composite Coatings at Elevated Temperatures

A TiAlN/Cr-Ni composite coating was fabricated on H13 hot work mold steel using a cathode ion arc plating and laser cladding. The surface and cross-sectional morphologies, chemical compositions, phases and surface roughness of obtained coating were analyzed using a scanning electron microscope, energy disperse spectroscopy, x-ray diffraction and atomic force microscope, respectively, and the bonding strength was measured using a scratch test. The friction-wear properties of TiAlN/Cr-Ni coating at 400, 500 and 600 °C were investigated using a ball-on-disc wear test. The results show that the TiAlN coating is primarily composed of c-TiN and c-AlN hard phases, and the bonding strength of TiAlN coating with the Cr-Ni coating is 22.15 N. The average coefficients of friction of TiAlN/Cr-Ni coating at 400, 500 and 600 °C are 0.458, 0.318 and 0.449, respectively, and the corresponding wear rates are 0.329 × 10{sup −3}, 0.384 × 10{sup −3} and 0.205 × 10{sup −3} mm{sup 3} N{sup −1} s{sup −1}, respectively, and the wear mechanism includes adhesive wear and oxidation wear.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Multi-probe microstructure tracking during heat treatment without an in-situ setup: Case studies on martensitic steel, dual phase steel and β-Ti alloy

In-situ scanning electron microscopy observations of the microstructure evolution during heat treatments are increasingly demanded due to the growing number of alloys with complex microstructures. Post-mortem characterization of the as-processed microstructures rarely provides sufficient insight on the exact route of the microstructure formation. On the other hand, in-situ SEM approaches are often limited due to the arising challenges upon using an in-situ heating setup, e.g. in (i) employing different detectors, (ii) preventing specimen surface degradation, or (iii) controlling and measuring the temperature precisely. Here, we explore and expand the capabilities of the “mid-way” solution by step-wise microstructure tracking, ex-situ, at selected steps of heat treatment. This approach circumvents the limitations above, as it involves an atmosphere and temperature well-controlled dilatometer, and high resolution microstructure characterization (using electron channeling contrast imaging, electron backscatter diffraction, atom probe tomography, etc.). We demonstrate the capabilities of this approach by focusing on three cases: (i) nano-scale carbide precipitation during low-temperature tempering of martensitic steels, (ii) formation of transformation-induced geometrically necessary dislocations in a dual-phase steel during intercritical annealing, and (iii) the partial recrystallization of a metastable β-Ti alloy. - Highlights: • A multi-probe method to track microstructures during heat treatment is developed. • It enables the analysis of various complex phenomena, even those at atomistic scale. • It circumvents some of the free surface effects of classical in-situ experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Electron tomography imaging methods with diffraction contrast for materials research

Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) enable the visualization of three-dimensional (3D) microstructures ranging from atomic to micrometer scales using 3D reconstruction techniques based on computed tomography algorithms. This 3D microscopy method is called electron tomography (ET) and has been utilized in the fields of materials science and engineering for more than two decades. Although atomic resolution is one of the current topics in ET research, the development and deployment of intermediate-resolution (non-atomic-resolution) ET imaging methods have garnered considerable attention from researchers. This research trend is probably not irrelevant due to the fact that the spatial resolution and functionality of 3D imaging methods of scanning electron microscopy (SEM) and X-ray microscopy have come to overlap with those of ET. In other words, there may be multiple ways to carry out 3D visualization using different microscopy methods for nanometer-scale objects in materials. From the above standpoint, this review paper aims to (i) describe the current status and issues of intermediate-resolution ET with regard to enhancing the effectiveness of TEM/STEM imaging and (ii) discuss promising applications of state-of-the-art intermediate-resolution ET for materials research with a particular focus on diffraction contrast ET for crystalline microstructures (superlattice domains and dislocations) including a demonstration of in situ dislocation tomography.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Study of (DNPs){sub x}/CuTl-1223 Nanoparticle-Superconductor Composites

Sol-gel and solid-state reaction methods were used to synthesize diamond nanoparticles (DNPs) and (DNPs){sub x}/CuTl-1223 (x = 0, 0.25, 0.50, and 1.00 wt.%) nanoparticle-superconductor composites, respectively. Effects of these DNPs on structural, morphological, compositional, and transport properties of CuTl-1223 superconducting phase were investigated by different experimental techniques such as X-ray diffraction (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM), and resistivity versus temperature (R-T) measurements. The unchanged crystal structure and stoichiometry of host CuTl-1223 superconducting matrix with addition of DNPs gave evidence about the dispersion of nanoparticles at the grain boundaries of the host matrix, which may heal up the inter-granular voids and pores resulting in enhanced inter-grain connectivity. Critical transition temperature T{sub c} (0) and hole concentration of CuTl-1223 superconductor were observed to be increased with addition of DNPs up to a certain optimum value (i.e. x = 0.5 wt.%).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2017

Temperature dependent solvothermal synthesis of Cu-Sb-S nanoparticles with tunable structural and optical properties

Highlights: • Cu{sub 3}SbS{sub 4} and CuSbS{sub 2} nanoparticles have been synthesized. • Solvothermal and drop casting method have been used. • Reaction temperature, Ethylene glycol and Polyvinylpyrrolidone plays major role. • Nanoparticles structure, morphology and optical properties have been characterized. • Famatinite and Chalcostibite thin films have been electrically Characterized. - Abstract: Copper based chalcogenide nanoparticles were synthesized by convenient solvothermal method using ethylene glycol as solvent and Polyvinylpyrrolidone as surfactant, followed by deposition of thin films using drop casting method. Here, the reactions were performed at different temperature from 200 °C to 240 °C in steps of 10 °C. Systematic investigation revealed that as temperature increases significant changes were occurring on the crystal structure, optical properties and electrical performance of the material. The influence of different temperature was responsible for the formation of pure Cu{sub 3}SbS{sub 4} to CuSbS{sub 2} nanoparticles. The obtained nanopowders and deposited films were characterized by X-ray diffraction, Raman analysis, high resolution transmission electron microscope, field emission scanning electron microscope with energy dispersive spectrometer, UV–Vis–NIR diffuse reflectance spectroscopy and hall measurement. Optical and electrical studies revealed that nanoparticles were in the range of 0.88–1.45 eV with p-type conductivity, indicating their potential application as a p-type absorber layer in thin film solar cells.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Fabrication of transparent cellulose acetate/graphene oxide nanocomposite film for UV shielding

In this work, we have fabricated transparent cellulose acetate/graphene oxide nanocomposite (CAGONC) films for ultraviolet radiations (UVR) shielding. Graphene oxide (GO) was synthesized by modified Hummer’s method and CAGONC films were fabricated by solvent casting method. The films were analyzed using characterization techniques like x-ray diffraction (XRD), energy dispersive x-ray (EDX) equipped scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy and ultra-violet visible (UV-VIS) spectroscopy. Four films were prepared by varying the wt% of GO (0.1wt%, 0.2wt% and 0.3wt%) with respect to cellulose acetate (CA). UV-vis measurements exhibit optical transparency in the range of 76-99% for visible light while ultra-violet radiation was substantially shielded.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Preparation and characterization of PVP-PVA–ZnO blend polymer nano composite films

Flexible self-standing films of PVP-PVA blend composites are prepared by using ZnO as a nano filler at different concentrations. The structural, compositional, morphological and optical studies made with the help of X-ray diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Scanning electron microscope (SEM), Atomic Force Microscopy (AFM), Ultraviolet-visible spectroscopy (UV-vis) and Photoluminescence (PL) spectra are presented in this paper. The results of XRD indicate that ZnO nanoparticles are formed with hexagonal phase in the polymeric matrix. SEM images show the dispersion of ZnO nano filler in the polymer matrix. UV–vis spectra reveal that the absorption peak is centered around 235 nm and 370 nm for the nano composite films. The blue shift is observed with decrease in the concentration of the nano filler. PL spectra shows the excitation wavelength is given at 320 nm.The emission peaks were observed at 383 nm ascribing to the electronic transitions between valence band and conduction band and the peak at 430 nm.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

The 4D Camera: An 87 kHz Direct Electron Detector for Scanning/Transmission Electron Microscopy

We describe the development, operation, and application of the 4D Camera—a 576 by 576 pixel active pixel sensor for scanning/transmission electron microscopy which operates at 87,000 Hz. The detector generates data at ~480 Gbit/s which is captured by dedicated receiver computers with a parallelized software infrastructure that has been implemented to process the resulting 10–700 Gigabyte-sized raw datasets. The back illuminated detector provides the ability to detect single electron events at accelerating voltages from 30 to 300 kV. Through electron counting, the resulting sparse data sets are reduced in size by 10--300× compared to the raw data, and open-source sparsity-based processing algorithms offer rapid data analysis. The high frame rate allows for large and complex scanning diffraction experiments to be accomplished with typical scanning transmission electron microscopy scanning parameters.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Synthesis and characterization of Pt(Cu 0.67 Sn 0.33 )

Pt(Cu 0.67 Sn 0.33 ) has recently been found in a natural sample. In order to be able to characterize this new ternary compound, we synthesized it from the elements. Samples were characterized by X-ray powder diffraction, differential scanning calorimetry, thermal relaxation calorimetry, and scanning electron microscopy studies. Density functional theory-based model calculations complemented the experimental studies. Pt(Cu 0.67 Sn 0.33 )was already formed at a relatively low temperature of 773 K. Rietveld refinement of Pt(Cu 0.67 Sn 0.33 ) has been carried out in CuAu-type or L1 0 -type structure, space group P4/mmm, with Pt on 0,0,0 and disordered Cu and Sn on 1/2, 1/2, 1/2 and Z = 1. The lattice parameters are a = 2.823(1) Å, c = 3.64(1) Å, and V = 29.00(4) Å which are in good agreement with values obtained earlier on the natural sample and with the results of DFT calculations. The vibrational entropy for Pt(Cu 0.67 Sn 0.33 ) is $S_{298.15}^{vib}$ = 79.9(7) J mol -1 K -1 . The pressure dependence up to 36(2) GPa of the unit-cell volume and the lattice parameters and unit-cell volume have been obtained by synchrotron based powder diffraction using a diamond anvil cell. A fit of a 3rd-order Birch–Murnaghan equation of state to the Pt(Cu 0.67 Sn 0.33 )) (p,V)-data results in a bulk modulus of B 0 = 215(27) GPa and B' = 5(2).

36 MATERIALS SCIENCE↗
DOE OSTI2018

Mechanical behavior and texture development of over-aged and solution treated Al-Cu-Mg alloy during multi-directional forging

The effects of initial heat treatments, i.e. solution treating and over ageing, on deformation behavior of an age hardenable Al-Cu-Mg alloy, including mechanical properties and texture evolution, during multi-directional forging (MDF) are investigated. Hardness measurements, electron back scatter diffraction (EBSD) maps, and differential scanning calorimetry (DSC) are carried out. Mechanical behaviors of the alloy in terms of compressive stress and hardness test after MDF are investigated. In both solution treated and over-aged alloys, the compressive stress during MDF shows an increase up to the second pass, and by further straining the flow stress is decreased. However, shear and deformation bands are formed in both solution treated and over-aged alloys, the density of these instabilities in the solution treated alloy is higher than that in over-aged alloy. In the solution treated alloy, not only large particles induce deformation bands, but also the dynamically formed GPB zones/Cu-Mg co-clusters. Texture analysis shows that the shear component of C {001}<110> (Φ{sub 1} = 90°, Φ = 0°, Φ{sub 2} = 45°) is developed with 18 mrd during MDF of the over-aged alloy. In the solution treated alloy, due to the high density of deformation bands and different microchemistry of the matrix in comparison with that of the over-aged alloy, the Copper type texture component {112}<111> (Φ{sub 1} = 90°, Φ = 35°, Φ{sub 2} = 45°) is developed with 11 mrd.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Catalytic Activity of Li{sub 1+x}Hf{sub 2–x}In{sub x}(PO{sub 4}){sub 3}-Based NASICON-Type Materials for Ethanol Conversion Reactions

Li{sub 1+} {sub x}Hf{sub 2–x}In{sub x}(PO{sub 4}){sub 3} (x = 0, 0.05, 0.1) materials have been prepared by solid-state reactions and characterized by X-ray diffraction, low-temperature nitrogen adsorption measurements, and scanning electron microscopy. The materials consist of NASICON-type lithium hafnium double phosphates with a hexagonal structure. Milling in a planetary mill has been found to increase the specific surface area of the Li{sub 1+} {sub x}Hf{sub 2–x}In{sub x}(PO{sub 4}){sub 3} materials by almost one order of magnitude (from 1.5 to 13 m{sup 2}/g in the case of LiHf{sub 2}(PO{sub 4}){sub 3}). The materials with a larger surface area exhibit catalytic activity for ethanol dehydration reactions and are less active for ethanol dehydrogenation. Ethanol conversion predominantly yields diethyl ether at low temperatures and ethylene at higher temperatures. The diethyl ether selectivity of the catalytic processes reaches 85% at 350°C, with 60% conversion, and the ethylene selectivity reaches 96% at 510°C, with 100% conversion. Indium doping raises the high-temperature acetaldehyde selectivity from 4 to 8% and leads to the formation of C{sub 4} hydrocarbons as reaction products. C{sub 4} selectivity reaches 15 and 17% in the case of the Li{sub 1.05}Hf{sub 1.95}In{sub 0.05}(PO{sub 4}){sub 3} and Li{sub 1.1}Hf{sub 1.9}In{sub 0.1}(PO{sub 4}){sub 3} materials, respectively (420°C, 97 and 92% conversion, respectively).

36 MATERIALS SCIENCE↗
DOE OSTI2021

A study on the creep behavior of alloy 709 using in-situ scanning electron microscopy

In this research, an experimental evaluation of creep properties of Alloy 709 in the temperature range of 750–850 °C was undertaken. Alloy 709 is a novel austenitic stainless steel with 20% Cr and 25% Ni by wt% that was developed for application in structural components of nuclear power plants. Creep rupture tests were conducted in an in-situ heating-loading and Scanning Electron Microscope (SEM) unit equipped with Electron Backscatter Diffraction (EBSD) detector and Energy Dispersive Spectroscopy (EDS). “Real-time” creep damage mechanisms of Alloy 709 at various stresses and temperatures using a flat, un-notched sample with continuously reducing cross-section is studied so that the failure and maximum creep damage occurred at the center of the sample where the in-situ SEM imaging could be focused. Accelerated creep tests at temperatures and stresses above service conditions were performed by employing multiple blocks of constant loads where the loads were increased once the sample attained constant creep rate, indicating a secondary creep regime. This technique ensures multiple data points can be obtained from the same test, saves the time required for an otherwise long-term creep test and usage of SEM. Further, Coincident Site Lattice (CSL) boundary maps were collected as control maps before testing, and the grain boundaries were observed during the creep test to understand the effect of grain boundary character on the creep damage mechanism. Void growth, grain boundary separation, and sliding were found to be the main creep mechanisms whose rate is dependent on stress and temperature. Failure mechanisms studied on the fracture surface using SEM fractography were correlated to the sample surface observations to create complementary information to better understand the underline creep mechanism of Alloy 709.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Fabrication and characterization of microstructure of stainless steel matrix composites containing up to 25 vol% NbC

AISI 440 stainless steels reinforced with various volume fractions of niobium carbide (NbC) particles of up to 25 vol% were fabricated in-situ using an argon arc furnace and then heat-treated to produce a martensitic matrix. Optical and scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and electron back-scatter diffraction (EBSD) techniques were used to analyze the microstructure, phases and composition of these composites. Interestingly, it was found that Chinese-script NbC could nucleate on existing primary NbC particles creating NbC clusters with complex microstructures. Additionally, hardness tests were used to evaluate viability in mining and mineral processing applications. The increase in NbC content resulted in an overall increase in the hardness of the composites while causing a marginal decrease in the amount of Cr in solid solution with the matrix, which could be a concern for corrosion resistance. The latter was due to the fact that the NbC lattice could dissolve a minor amount of Cr. Thermodynamic simulations also attributed this to a slight increase in M{sub 7}C{sub 3} precipitation. Nonetheless, these novel composites show great promise for applications in wear and corrosive environments. - Highlights: •Stainless steels reinforced with NbC particles of up to 25 vol% were fabricated. •NbC was formed in-situ in the steels using an arc melter. •Martensitic transformation of the matrix of each sample was achieved. •NbC reinforcements increased the bulk hardness values of the steels. •Dissolved Cr in the matrix of each sample was sufficient for passivity in theory.

36 MATERIALS SCIENCE↗
DOE OSTI2024

High‐speed 4‐dimensional scanning transmission electron microscopy using compressive sensing techniques

Abstract Here we show that compressive sensing allows 4‐dimensional (4‐D) STEM data to be obtained and accurately reconstructed with both high‐speed and reduced electron fluence. The methodology needed to achieve these results compared to conventional 4‐D approaches requires only that a random subset of probe locations is acquired from the typical regular scanning grid, which immediately generates both higher speed and the lower fluence experimentally. We also consider downsampling of the detector, showing that oversampling is inherent within convergent beam electron diffraction (CBED) patterns and that detector downsampling does not reduce precision but allows faster experimental data acquisition. Analysis of an experimental atomic resolution yttrium silicide dataset shows that it is possible to recover over 25 dB peak signal‐to‐noise ratio in the recovered phase using 0.3% of the total data. Lay abstract : Four‐dimensional scanning transmission electron microscopy (4‐D STEM) is a powerful technique for characterizing complex nanoscale structures. In this method, a convergent beam electron diffraction pattern (CBED) is acquired at each probe location during the scan of the sample. This means that a 2‐dimensional signal is acquired at each 2‐D probe location, equating to a 4‐D dataset. Despite the recent development of fast direct electron detectors, some capable of 100kHz frame rates, the limiting factor for 4‐D STEM is acquisition times in the majority of cases, where cameras will typically operate on the order of 2kHz. This means that a raster scan containing 256^2 probe locations can take on the order of 30s, approximately 100‐1000 times longer than a conventional STEM imaging technique using monolithic radial detectors. As a result, 4‐D STEM acquisitions can be subject to adverse effects such as drift, beam damage, and sample contamination. Recent advances in computational imaging techniques for STEM have allowed for faster acquisition speeds by way of acquiring only a random subset of probe locations from the field of view. By doing this, the acquisition time is significantly reduced, in some cases by a factor of 10‐100 times. The acquired data is then processed to fill‐in or inpaint the missing data, taking advantage of the inherently low‐complex signals which can be linearly combined to recover the information. In this work, similar methods are demonstrated for the acquisition of 4‐D STEM data, where only a random subset of CBED patterns are acquired over the raster scan. We simulate the compressive sensing acquisition method for 4‐D STEM and present our findings for a variety of analysis techniques such as ptychography and differential phase contrast. Our results show that acquisition times can be significantly reduced on the order of 100‐300 times, therefore improving existing frame rates, as well as further reducing the electron fluence beyond just using a faster camera.

Robinson, Alex W.↗
DOE OSTI2016

Enhanced field emission properties of tilted graphene nanoribbons on aggregated TiO{sub 2} nanotube arrays

Highlights: • Graphene nanoribbons (GNBs) slanted on aggregate TiO{sub 2} nanotube (A-TNTs) as field-emitters. • Turn-on electric field and field enhancement factor β are dependent on the substrate morphology. • Various quantities of GNRs are deposited on top of A-TNTs (GNRs/A-TNTs) with different morphologies. • With an increase of GNBs compositions, the specimens' turn-on electric field is reduced to 2.8 V/μm. • The field enhancement factor increased rapidly to about 1964 with the addition of GNRs. - Abstract: Graphene nanoribbons (GNRs) slanted on aggregate TiO{sub 2} nanotube arrays (A-TNTs) with various compositions as field-emitters are reported. The morphology, crystalline structure, and composition of the as-obtained specimens were characterized by field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and Raman spectrometry. The dependence of the turn-on electric field and the field enhancement factor β on substrate morphology was studied. An increase of GNRs reduces the specimens’ turn-on electric field to 2.8 V/μm and the field enhancement factor increased rapidly to about 1964 with the addition of GNRs. Results show a strong dependence of the field emission on GNR composition aligned with the gradient on the top of the A-TNT substrate. Enhanced FE properties of the modified TNTs can be mainly attributed to their improved electrical properties and rougher surface morphology.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Structural investigation of cooperite (PtS) crystals

The single-crystal structure of cooperite, a natural platinum sulfide PtS, is studied by X-ray diffraction supported by high-resolution scanning transmission electron microscopy and X-ray spectrum microanalysis. It is found that, in addition to the main reflections corresponding to the known tetragonal cell (a = 3.47 and c = 6.11 Å; space group P4{sub 2}/mmc), many weak reflections with intensities I ≤ 60σ(I) are clearly observed. These reflections fit the tetragonal cell (space group I4/mmm) with doubled parameters. In structures with small (P4{sub 2}/mmc) and large (I4/mmm) cells, the S atoms occupy statistically two special positions. It is shown that the chemical composition of the cooperite crystals deviates from the stoichiometric composition: sulfur-deficient specimens predominate.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗